CN112251606A - Distillation recovery method of waste mercury catalyst - Google Patents
Distillation recovery method of waste mercury catalyst Download PDFInfo
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- CN112251606A CN112251606A CN202011180317.XA CN202011180317A CN112251606A CN 112251606 A CN112251606 A CN 112251606A CN 202011180317 A CN202011180317 A CN 202011180317A CN 112251606 A CN112251606 A CN 112251606A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/009—General processes for recovering metals or metallic compounds from spent catalysts
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B43/00—Obtaining mercury
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a distillation recovery method of a waste mercury catalyst, which comprises the following steps: putting the waste mercury catalyst into a sodium hydroxide solution, and heating to enable mercury chloride in the waste mercury catalyst to react with sodium hydroxide so as to convert the mercury chloride into mercury oxide and obtain a pretreated waste material; placing the pretreated waste into a distillation furnace, and heating to decompose oxidized mercury in the pretreated waste into mercury vapor; introducing mercury vapor into an air condenser for indirect condensation, so that most of the mercury vapor forms liquid metal mercury and then falls into a lower mercury collecting tank for storage, and the residual mercury vapor is condensed by a multi-tube condenser to obtain liquid metal mercury and mercury soot which enters a lower mercury collecting tank; tail gas is absorbed by modified active carbon, and the absorbed tail gas is discharged after being washed by a sodium sulfide solution. Compared with the prior art, the modified activated carbon is adopted to adsorb the tail gas after the distillation of the waste mercury catalyst, so that the mercury absorption capacity of the activated carbon can be improved, and the cleanliness of the tail gas can be greatly improved.
Description
Technical Field
The invention relates to the technical field of industrial waste recovery treatment, in particular to a distillation recovery method of a waste mercury catalyst.
Background
When the calcium carbide method is adopted to produce the chloroethylene, a mercury catalyst with the mercury chloride content of up to 10 wt% is needed to be adopted as a catalyst to catalyze acetylene and hydrogen chloride gas to synthesize the chloroethylene. The mercury catalyst is a catalyst with active carbon as carrier and mercuric chloride as active matter. After the mercury catalyst is used for a certain period of time, the activity of the mercury catalyst is reduced and the mercury catalyst needs to be replaced, and the replaced waste mercury catalyst generally contains about 2-5% of mercury chloride. At present, China is the largest PVC producing country in the world, and a large amount of waste mercury catalysts are generated in the production process due to HgCl2Has the strong toxicity of the raw materials,and the mercury catalyst is volatile and soluble in water, so that the direct discharge of the replaced mercury catalyst can cause serious environmental pollution, and if the mercury catalyst is stacked or stored for a long time, the environmental pollution and the potential safety hazard are easily caused. Therefore, mercury in the waste mercury catalyst needs to be recovered to avoid the mercury from entering the environment and causing harm to human health.
The contact recovery treatment method of the waste mercury is roughly divided into a wet method and a dry method, the wet method recovery usually adopts an alkali soaking-roasting method, the recovery rate is low, the recovery method cost is higher, a large amount of water resource waste is caused in the recovery process, and the recovery process is longer, the time consumption is longer, so the use is less. The dry treatment is to carry out chemical pretreatment on the waste mercury catalyst and to carry out HgCl treatment on the waste mercury catalyst2And the mercury is converted into mercury oxide, then the mercury oxide is placed in a metal can, the metal can is heated to 700-800 ℃ to be decomposed into mercury vapor, and the mercury vapor is condensed to recover the metal mercury.
However, the waste gas after mercury vapor condensation in the dry treatment is directly discharged by adopting the conventional purification treatment, the treatment capacity of the waste gas is large, and even if the waste gas is discharged after reaching the standard, the total discharge amount is accumulated, so that the serious environmental pollution is also generated.
Disclosure of Invention
In order to solve the technical problem, the invention provides a distillation recovery method of waste mercury catalyst for improving the recovery cleanliness.
The invention provides a distillation recovery method of a waste mercury catalyst, which comprises the following steps:
putting the waste mercury catalyst into a sodium hydroxide solution, and heating to enable mercury chloride in the waste mercury catalyst to react with sodium hydroxide so as to convert the mercury chloride into mercury oxide and obtain a pretreated waste material;
placing the pretreated waste into a distillation furnace, and heating to decompose oxidized mercury in the pretreated waste into mercury vapor;
introducing mercury vapor into an air condenser for indirect condensation, so that most of the mercury vapor forms liquid metal mercury and then falls into a lower mercury collecting tank for storage, and the residual mercury vapor is condensed by a multi-tube condenser to obtain liquid metal mercury and mercury soot which enters a lower mercury collecting tank;
tail gas is absorbed by modified active carbon, and the absorbed tail gas is discharged after being washed by a sodium sulfide solution;
the preparation process of the modified activated carbon comprises the following steps: mixing activated carbon and hydrogen peroxide under heating and ultrasonic oscillation; and carrying out post-treatment to obtain the modified activated carbon.
Preferably, the waste mercury catalyst is placed in a sodium hydroxide solution, and mercury chloride in the waste mercury catalyst reacts with the sodium hydroxide by heating, so that the mercury chloride is converted into mercury oxide to obtain a pretreated waste material; the method comprises the following steps:
and (2) placing the waste mercury catalyst into a sodium hydroxide solution with the mass fraction of 30-40%, heating to 80-90 ℃, stirring for 1.5-2.5 h, and reacting the mercuric chloride in the waste mercury catalyst with the sodium hydroxide to convert the mercuric chloride into mercuric oxide to obtain the pretreated waste.
Preferably, after the step of placing the waste mercury catalyst in a sodium hydroxide solution, and reacting the mercury chloride in the waste mercury catalyst with the sodium hydroxide by heating, so as to convert the mercury chloride into mercury oxide, so as to obtain a pretreated waste material, the method further comprises:
and storing the pretreated waste for 72-96 h, so that the mercuric chloride in the pretreated waste is completely converted into mercuric oxide, and simultaneously, the water in the pretreated waste is leaked out.
Preferably, the pretreated waste is placed in a distillation furnace, and the temperature is increased to decompose oxidized mercury in the pretreated waste into mercury vapor; the method comprises the following steps:
and (3) placing the pretreated waste into a distillation furnace, heating to 700-800 ℃, and distilling for 8-12 h to decompose oxidized mercury in the pretreated waste into mercury vapor.
Preferably, the preparation process of the modified activated carbon is as follows: mixing the activated carbon and hydrogen peroxide according to the mass-to-volume ratio of 5g to 10-15 ml, heating at 50-70 ℃, and ultrasonically oscillating for 2-4 hours; standing, filtering, drying, washing and drying to obtain the modified activated carbon.
Preferably, the mass concentration of the hydrogen peroxide is 25-30%.
Preferably, the modified activated carbon after adsorbing the tail gas is placed in a distillation furnace, the temperature is raised to convert mercury adsorbed on the modified activated carbon into mercury vapor, and the desorbed modified activated carbon is obtained; and introducing mercury vapor into an air condenser for indirect condensation, so that most of the mercury vapor forms liquid metal mercury and then falls into a lower mercury collecting tank for storage, and the residual mercury vapor is condensed by a multi-tube condenser to obtain liquid metal mercury and mercury soot which enters a lower mercury collecting tank.
Preferably, the distillation waste residue and the fuel are mixed and then are roasted at high temperature, and roasting flue gas is discharged after combustion, cooling, dust collection, modified activated carbon adsorption and desulfurization.
Preferably, the high-temperature roasting temperature is 1100-1200 ℃, and the roasting time is 1-2 h.
Preferably, the mass ratio of the distillation waste residue to the fuel is 1: 0.1-0.2.
According to the distillation recovery method of the waste mercury catalyst, the tail gas after distillation of the waste mercury catalyst is adsorbed by the modified activated carbon, and the pore structure and the surface functional group of the activated carbon are changed by thermal modification and ultrasonic modification by adopting a hydrogen peroxide modification method, so that the obtained modified activated carbon has high mercury adsorption performance, and the cleanliness of the tail gas can be greatly improved.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the present application will be clearly and completely described below with reference to the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments.
It will be understood that when an element is referred to as being "fixed" or "disposed" on another element, it can be directly on the other element or be indirectly disposed on the other element; when an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
It will be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used merely to facilitate describing the application and to simplify the description, and do not indicate or imply that the referenced devices or elements must be in a particular orientation, constructed and operated in a particular orientation, and are therefore not to be considered limiting of the application.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, the meaning of a plurality of or a plurality of is two or more unless specifically limited otherwise.
The embodiment of the invention provides a distillation recovery method of a waste mercury catalyst, which comprises the following steps:
s110, placing the waste mercury catalyst into a sodium hydroxide solution, and heating to enable mercury chloride in the waste mercury catalyst to react with sodium hydroxide so as to convert the mercury chloride into mercury oxide and obtain a pretreated waste material;
s120, placing the pretreated waste into a distillation furnace, and heating to decompose oxidized mercury in the pretreated waste into mercury vapor;
s130, introducing mercury vapor into an air condenser for indirect condensation, so that most of mercury vapor forms liquid metal mercury and then falls into a lower mercury collecting tank for storage, and the residual mercury vapor is condensed by a multi-tube condenser to obtain liquid metal mercury and mercury soot which enter a lower mercury collecting tank;
s140, adsorbing the tail gas by using modified activated carbon, and washing the adsorbed tail gas by using a sodium sulfide solution and then discharging the tail gas;
the preparation process of the modified activated carbon comprises the following steps: mixing activated carbon and hydrogen peroxide under heating and ultrasonic oscillation; and carrying out post-treatment to obtain the modified activated carbon.
According to the distillation recovery method of the waste mercury catalyst, the tail gas after distillation of the waste mercury catalyst is adsorbed by the modified activated carbon, and the pore diameter structure and the surface functional group of the activated carbon are changed by thermal modification and ultrasonic modification by a hydrogen peroxide modification method, so that the obtained modified activated carbon has high mercury adsorption performance, and the cleanliness of the tail gas can be greatly improved.
Specifically, in the above embodiment, the specific process of S110 is as follows:
and (2) placing the waste mercury catalyst into a sodium hydroxide solution with the mass fraction of 30-40%, heating to 80-90 ℃, stirring for 1.5-2.5 h, and reacting the mercuric chloride in the waste mercury catalyst with the sodium hydroxide to convert the mercuric chloride into mercuric oxide to obtain the pretreated waste.
Further, in the above embodiment, the following steps are further included between S110 and S120:
and storing the pretreated waste for 72-96 h, so that the mercuric chloride in the pretreated waste is completely converted into mercuric oxide, and simultaneously, the water in the pretreated waste is leaked out.
Further, in the above embodiment, the specific process of S120 is as follows:
and (3) placing the pretreated waste into a distillation furnace, heating to 700-800 ℃, and distilling for 8-12 h to decompose oxidized mercury in the pretreated waste into mercury vapor.
Further, in the above examples, the specific preparation process of the modified activated carbon is as follows: mixing the activated carbon and hydrogen peroxide according to the mass-to-volume ratio of 5g to 10-15 ml, heating at 50-70 ℃, and ultrasonically oscillating for 2-4 hours; standing, filtering, drying, washing and drying to obtain the modified activated carbon.
Furthermore, in the embodiment, the mass concentration of the hydrogen peroxide is 25-30%.
Furthermore, in the above embodiment, the modified activated carbon after adsorbing the tail gas is placed in a distillation furnace, and the temperature is raised to convert mercury adsorbed on the modified activated carbon into mercury vapor, so as to obtain desorbed modified activated carbon; and introducing mercury vapor into an air condenser for indirect condensation, so that most of the mercury vapor forms liquid metal mercury and then falls into a lower mercury collecting tank for storage, and the residual mercury vapor is condensed by a multi-tube condenser to obtain liquid metal mercury and mercury soot which enters a lower mercury collecting tank.
Therefore, the desorbed modified activated carbon can be repeatedly used, the utilization rate of the modified activated carbon is improved, and the treatment cost of the waste mercury catalyst is saved.
Furthermore, in the above embodiment, the distillation waste residue and the fuel are mixed and then calcined at high temperature, and the calcined flue gas is discharged after combustion, cooling, dust collection, modified activated carbon adsorption and desulfurization.
And (3) carrying out high-temperature roasting treatment on the waste mercury catalyst residue produced by the distillation furnace, burning and decomposing active carbon and other components in the residue at high temperature, and burning the roasted flue gas to further burn the unburned combustible gas in the roasting furnace so as to remove toxic and harmful components in the flue gas. The flue gas after burning is quenched to below 200 ℃, so that secondary synthesis of dioxin is avoided. The cooled flue gas is subjected to dust collection and modified active carbon to adsorb toxic and harmful gases in the flue gas. And (3) performing secondary spraying desulfurization treatment on the sulfur-containing flue gas subjected to the adsorption treatment by using the activated carbon, so that the flue gas content reaches the standard and is discharged. Therefore, the purpose that the residues generated by the distillation furnace are converted into common solid waste residues and the flue gas is properly treated is realized, and the problem that the residues pollute the environment secondarily in the traditional treatment process is solved.
Furthermore, in the above embodiment, the high-temperature baking temperature is 1100-1200 ℃ and the baking time is 1-2 h.
Furthermore, in the above embodiment, the mass ratio of the distillation waste residue to the fuel is 1: 0.1-0.2.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for distilling and recovering waste mercury catalyst is characterized by comprising the following steps:
putting the waste mercury catalyst into a sodium hydroxide solution, and heating to enable mercury chloride in the waste mercury catalyst to react with sodium hydroxide so as to convert the mercury chloride into mercury oxide and obtain a pretreated waste material;
placing the pretreated waste into a distillation furnace, and heating to decompose oxidized mercury in the pretreated waste into mercury vapor;
introducing mercury vapor into an air condenser for indirect condensation, so that most of the mercury vapor forms liquid metal mercury and then falls into a lower mercury collecting tank for storage, and the residual mercury vapor is condensed by a multi-tube condenser to obtain liquid metal mercury and mercury soot which enters a lower mercury collecting tank;
tail gas is absorbed by modified active carbon, and the absorbed tail gas is discharged after being washed by a sodium sulfide solution;
the preparation process of the modified activated carbon comprises the following steps: mixing activated carbon and hydrogen peroxide under heating and ultrasonic oscillation; and carrying out post-treatment to obtain the modified activated carbon.
2. The method for recovering the waste mercury catalyst through distillation as claimed in claim 1, wherein the waste mercury catalyst is placed in a sodium hydroxide solution, and the mercuric chloride in the waste mercury catalyst is reacted with the sodium hydroxide through heating, so that the mercuric chloride is converted into mercuric oxide, thereby obtaining a pretreated waste; the method comprises the following steps:
and (2) placing the waste mercury catalyst into a sodium hydroxide solution with the mass fraction of 30-40%, heating to 80-90 ℃, stirring for 1.5-2.5 h, and reacting the mercuric chloride in the waste mercury catalyst with the sodium hydroxide to convert the mercuric chloride into mercuric oxide to obtain the pretreated waste.
3. The method for recovering the mercury catalyst as claimed in claim 1, further comprising the steps of:
and storing the pretreated waste for 72-96 h, so that the mercuric chloride in the pretreated waste is completely converted into mercuric oxide, and simultaneously, the water in the pretreated waste is leaked out.
4. The method of claim 1, wherein the pretreated waste material is placed in a distillation furnace, and the temperature is raised to decompose oxidized mercury in the pretreated waste material into mercury vapor; the method comprises the following steps:
and (3) placing the pretreated waste into a distillation furnace, heating to 700-800 ℃, and distilling for 8-12 h to decompose oxidized mercury in the pretreated waste into mercury vapor.
5. The method for recovering the waste mercury catalyst as defined in any one of claims 1 to 4, wherein the modified activated carbon is prepared by the following steps: mixing the activated carbon and hydrogen peroxide according to the mass-to-volume ratio of 5g to 10-15 ml, heating at 50-70 ℃, and ultrasonically oscillating for 2-4 hours; standing, filtering, drying, washing and drying to obtain the modified activated carbon.
6. The method for recovering the waste mercury catalyst through distillation as claimed in claim 5, wherein the mass concentration of the hydrogen peroxide is 25-30%.
7. The method for recovering the waste mercury catalyst according to any one of claims 1 to 4, wherein the modified activated carbon after adsorbing the tail gas is placed in a distillation furnace, and the temperature is raised to convert the mercury adsorbed on the modified activated carbon into mercury vapor and obtain the desorbed modified activated carbon; and introducing mercury vapor into an air condenser for indirect condensation, so that most of the mercury vapor forms liquid metal mercury and then falls into a lower mercury collecting tank for storage, and the residual mercury vapor is condensed by a multi-tube condenser to obtain liquid metal mercury and mercury soot which enters a lower mercury collecting tank.
8. The method for recovering the waste mercury catalyst according to any one of claims 1 to 4, wherein the waste residue is mixed with a fuel and then calcined at a high temperature, and the calcined flue gas is discharged after combustion, cooling, dust collection, modified activated carbon adsorption and desulfurization.
9. The method for recovering waste mercury catalyst as defined in claim 8, wherein the high-temperature calcination is performed at 1100-1200 ℃ for 1-2 hours.
10. The method of claim 8, wherein the mass ratio of the waste residue to the fuel is 1: 0.1-0.2.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011180317.XA CN112251606A (en) | 2020-10-29 | 2020-10-29 | Distillation recovery method of waste mercury catalyst |
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| CN202011180317.XA CN112251606A (en) | 2020-10-29 | 2020-10-29 | Distillation recovery method of waste mercury catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113174498A (en) * | 2021-04-20 | 2021-07-27 | 南通润启环保服务有限公司 | Resource treatment and recovery method for waste mercury liquid and compounds |
| CN115433841A (en) * | 2022-08-31 | 2022-12-06 | 贵州万山天业绿色环保科技有限公司 | Method for recycling waste mercury catalyst |
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|---|---|---|---|---|
| US3537843A (en) * | 1967-04-04 | 1970-11-03 | Knapsack Ag | Process for recovering mercury from an inactive mercuric chloride/active carbon-catalyst |
| CN103223330A (en) * | 2013-05-13 | 2013-07-31 | 中国林业科学研究院林产化学工业研究所 | Preparation method of special modified active carbon for removing mercury |
| CN108559857A (en) * | 2018-04-23 | 2018-09-21 | 喜德县良在硅业有限公司 | A kind of useless mercury catalyst mercury recycling and slag harmlessness treatment process |
| CN110144462A (en) * | 2019-05-14 | 2019-08-20 | 贵州万山天业绿色环保科技有限公司 | A kind of mercury processing electrothermic retorting technique |
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2020
- 2020-10-29 CN CN202011180317.XA patent/CN112251606A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3537843A (en) * | 1967-04-04 | 1970-11-03 | Knapsack Ag | Process for recovering mercury from an inactive mercuric chloride/active carbon-catalyst |
| CN103223330A (en) * | 2013-05-13 | 2013-07-31 | 中国林业科学研究院林产化学工业研究所 | Preparation method of special modified active carbon for removing mercury |
| CN108559857A (en) * | 2018-04-23 | 2018-09-21 | 喜德县良在硅业有限公司 | A kind of useless mercury catalyst mercury recycling and slag harmlessness treatment process |
| CN110144462A (en) * | 2019-05-14 | 2019-08-20 | 贵州万山天业绿色环保科技有限公司 | A kind of mercury processing electrothermic retorting technique |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113174498A (en) * | 2021-04-20 | 2021-07-27 | 南通润启环保服务有限公司 | Resource treatment and recovery method for waste mercury liquid and compounds |
| CN115433841A (en) * | 2022-08-31 | 2022-12-06 | 贵州万山天业绿色环保科技有限公司 | Method for recycling waste mercury catalyst |
| CN115433841B (en) * | 2022-08-31 | 2023-08-04 | 贵州万山天业绿色环保科技有限公司 | Method for recycling waste mercury catalyst |
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